WSLH Organic Section

Organic Chemistry Section
Tissue Analysis

Wildlife & Fish Tissue | Water | Serum | Sediments & Soils

Section 1410: Pesticide and PCB Residues in Tissue

Rev. 3.1 -- August 1, 2003

1410.1 Scope and Application

This method may be used to analyze fish and wildlife tissue for various chlorinated pesticides and PCBs. Analysis for PCBs includes: Aroclor mixtures by packed column (section A, below), individual congeners contained in the "Mullin" mix by capillary/ECD (section B), and selected co-planar (or toxic) congeners by multi-dimensional GC/ECD (section C).

Pesticides and PCBs by Packed and Capillary Column Chromatography

Compound	Report Limit µg/g	LOD µg/g	LOQ µg/g
Polychlorinated biphenyls		0.040	0.13
Dieldrin		0.020	0.064
o,p-DDE		0.030	0.095
p,p-DDE		0.030	0.095
o,p-DDD		0.040	0.13
p,p-DDD		0.040	0.13
o,p-DDD		0.040	0.13
p,p-DDT		0.040	0.13
cis-chlordane		0.020	0.064
trans-chlordane		0.020	0.064
cis-nonachlor		0.020	0.064
trans-nonachlor		0.020	0.064
Aldrin	0.05
Endrin	0.02
Hexachlorobenzene	0.01
alpha-BHC	0.01
gamma-BHC	0.01
oxychlordane	0.05
Methoxychlor	0.05
Toxaphene	1.0
Heptachlor epoxide	0.05

PCB Congeners by Capillary Column Chromatography

BZ # (e)	LOD (ng/g)	LOQ (ng/g)
#3	16.	53.
#4/10	3.4	11.
#7/9	0.60	2.0
#6	1.3	4.3
#8/5	3.3	11.
#19	1.0	3.3
#18	1.0	3.3
#15/17	1.5	5.0
#24/27	0.60	2.0
#16/32	1.7	5.7
#26	1.0	3.3
#25	1.0	3.3
#28/31	2.0	6.7
#33	1.0	3.3
#53	0.60	2.0
#51	0.60	2.0
#22	1.5	5.0
#45	0.80	2.7
#46	0.80	2.7
#52	0.90	3.0
#49	0.70	2.3
#47/48	1.2	4.0
#44	0.80	2.7
#37/42	1.2	4.0
#41/71/64	1.2	4.0
#40	0.80	2.7
#63	0.90	3.0
#74	0.70	2.3
#70/76	0.70	2.3
#66	1.2	4.0
#95	0.80	2.7
#91	0.90	3.0
#56/60	0.90	3.0
#92/84	1.7	5.7
#89	0.70	2.3
#101	0.70	2.3
#99	0.60	2.0
#83	0.60	2.0
#97	0.50	1.7
#87	0.70	2.3
#85	0.80	2.7
#136	2.0	6.7
#77/110	0.80	2.7
#82	0.60	2.0
#151	0.70	2.3
#135/144	1.0	3.3
#123/149	0.70	2.3
#118	1.0	3.3
#146	0.70	2.3
#132/153/105	1.0	3.3
#141	0.60	2.0
#137/176	0.70	2.3
#163/138	1.1	3.7
#158	3.3	11.
#178	1.0	3.3
#187/182	0.70	2.3
#183	0.70	2.3
#128	0.60	2.0
#167	0.90	3.0
#185	0.50	1.7
#174	0.70	2.3
#177	0.70	2.3
#202/171	0.50	1.7
#172	1.0	3.3
#180	0.80	2.7
#193	1.0	3.3
#199	0.70	2.3
#170/190	0.80	2.7
#198	0.80	2.7
#201	1.0	3.3
#203/196	1.7	5.7
#208/195	0.60	2.0
#207	0.50	1.7
#194	0.60	2.0
#206	0.60	2.0

"Toxic" PCB Congeners by Multidimensional Gas Chromatography

NOTE: The toxic congener list includes the twelve congeners in the World Health Organization (WHO) 1998 list, plus #180. There is overlap with the list in section B, which also includes PCBs #118, #167, and #180.

BZ # (e)	LOD (ng/g)	LOQ (ng/g)
#81	0.50	1.7
#77	0.50	1.7
#123	1.1	3.7
#114	0.50	1.7
#105	0.90	3.0
#126	0.60	2.0
#156	0.90	3.0
#157	0.60	2.0
#169	0.50	1.7
#189	0.60	2.0
#118	1.1	3.7
#167	0.80	2.7
#180	0.90	3.0

Poly-Brominated Diphenyl Ethers by Capillary Column GC

BZ # (e)	LOD (ng/g)	LOQ (ng/g)
#28	3.0	10.0
#47	3.0	10.0
#66	3.0	10.0
#85	3.5	12.0
#99	3.0	10.0
#100	3.0	10.0
#138	3.5	12.0
#153	3.5	12.0
#154	3.0	10.0

1410.2 Summary of Method

Tissue samples (fish and wildlife) are homogenized in a blender with dry ice and alllowed to stand overnight. Then approximately ten grams are combined with sodium sulfate and extracted with MeCl2. The lipid is removed by gel-permeation chromatography. In addition the extract may require additional clean-up or fractionation with silica-gel or florisil. The final extract or extracts are concentrated and injected onto a gas chromatograph equipped with an electron-capture detector. The type of column and GC used varies depending on particular analytes.

Section 1293: PCBs and Pesticides in Surface Water by XAD-2 Resin Extraction

Rev. 3.1 -- August 1, 2003

1293.1 Scope and Application

This method is used to determine congener specific PCB and Pesticide concentrations at trace levels in surface water. A multi-plate filtration system for collection of particulates, and an XAD-2 resin column for collection of dissolved PCBs is used. Water volumes of 80 L to 160 L can be analyzed by this method.

PCB Congeners by Capillary Column Chromatography

	80L		160L
BZ # (1)	LOD (MDL) ng/L	LOQ ng/L	LOD (MDL) ng/L	LOQ ng/L
#3	0.43	1.4	0.22	0.72
#4/10	0.050	0.17	0.025	0.083
#7/9	0.011	0.037	0.0055	0.018
#6	0.022	0.073	0.011	0.037
#8/5	0.049	0.16	0.024	0.080
#19	0.0070	0.023	0.0035	0.012
#18	0.014	0.047	0.0070	0.023
#15/17	0.030	0.10	0.015	0.050
#24/27	0.0070	0.023	0.0035	0.012
#16/32	0.022	0.073	0.011	0.037
#26	0.014	0.047	0.0070	0.023
#25	0.012	0.040	0.0060	0.020
#28/31	0.040	0.13	0.020	0.070
#33	0.015	0.050	0.0075	0.025
#53	0.0080	0.027	0.0040	0.013
#51	0.0070	0.023	0.0035	0.012
#22	0.022	0.073	0.011	0.037
#45	0.0090	0.030	0.0045	0.015
#46	0.0090	0.030	0.0045	0.015
#52	0.015	0.050	0.0075	0.025
#49	0.010	0.033	0.0050	0.017
#47/48	0.018	0.060	0.0090	0.030
#44	0.013	0.043	0.0065	0.022
#37/42	0.020	0.067	0.010	0.033
#41/71/64	0.020	0.067	0.010	0.033
#40	0.010	0.033	0.0050	0.017
#63	0.025	0.083	0.012	0.040
#74	0.013	0.043	0.0065	0.022
#70/76	0.025	0.083	0.012	0.040
#66	0.023	0.076	0.012	0.040
#95	0.012	0.040	0.0060	0.020
#91	0.011	0.037	0.0055	0.018
#56/60	0.016	0.053	0.0080	0.027
#92/84	0.024	0.080	0.012	0.040
#89	0.0060	0.020	0.0030	0.010
#101	0.011	0.037	0.0055	0.018
#99	0.0080	0.027	0.0040	0.013
#83	0.0090	0.030	0.0045	0.015
#97	0.0060	0.020	0.0030	0.010
#87	0.010	0.033	0.0050	0.017
#85	0.011	0.037	0.0055	0.018
#136	0.030	0.10	0.015	0.050
#77/110	0.022	0.073	0.011	0.037
#82	0.0070	0.023	0.0035	0.012
#151	0.010	0.033	0.0050	0.017
#135/144	0.013	0.043	0.0065	0.022
#123/149	0.010	0.033	0.0050	0.017
#118	0.016	0.053	0.0080	0.027
#146	0.011	0.037	0.0055	0.018
#132/153/105	0.020	0.067	0.010	0.033
#141	0.0080	0.027	0.0040	0.013
#137/176	0.013	0.043	0.0065	0.022
#163/138	0.022	0.073	0.011	0.037
#158	0.015	0.050	0.0075	0.025
#178	0.014	0.047	0.0070	0.023
#187/182	0.010	0.033	0.0050	0.017
#183	0.011	0.037	0.0055	0.018
#128	0.0090	0.030	0.0045	0.015
#167	0.012	0.040	0.0060	0.020
#185	0.0070	0.023	0.0035	0.012
#174	0.011	0.037	0.0055	0.018
#177	0.012	0.040	0.0060	0.020
#202/171	0.0080	0.027	0.0040	0.013
#172	0.015	0.050	0.0075	0.025
#180	0.013	0.043	0.0065	0.022
#193	0.015	0.050	0.0075	0.025
#199	0.0090	0.030	0.0045	0.015
#170/190	0.011	0.037	0.0055	0.018
#198	0.015	0.050	0.0075	0.025
#201	0.018	0.060	0.0090	0.030
#203/196	0.028	0.093	0.014	0.047
#208/195	0.0080	0.027	0.0040	0.013
#207	0.0070	0.023	0.0035	0.012
#194	0.011	0.037	0.0055	0.018
#206	0.0070	0.023	0.0035	0.012

Pesticide LODs and LOQs: 80 L and 160 L Water

	80L		160L
Compound	LOD (MDL) ng/L	LOQ ng/L	LOD (MDL) ng/L	LOQ ng/L
alpha-BHC	0.050	0.16	0.025	0.082
gamma-BHC (Lindane)	0.050	0.16	0.025	0.082
oxychlordane	0.019	0.063	0.010	0.033
gamma-chlordane	0.022	0.073	0.011	0.037
alpha-chlordane	0.021	0.070	0.010	0.033
trans-nonachlor	0.017	0.057	0.0085	0.028
p,p'DDD	0.050	0.16	0.025	0.082
cis-nonachlor	0.021	0.070	0.010	0.033
p,p'DDT	0.050	0.16	0.025	0.082
toxaphene	10.	33.	5.	16.
hexachlorobenzene (HCB)	0.0060	0.020	0.0030	0.010
p,p'DDE	0.030	0.10	0.015	0.050

1293.2 Summary of Method

Nominal volumes of 80L or 160L of surface water are filtered in the field through glass fiber filters held in a PentaPlate holder, then pumped through XAD-2 resin columns which adsorb dissolved organics. Filters and resin are separately soxhlet extracted, cleaned up using Florisil, silica gel, and concentrated sulfuric acid, and analyzed by capillary column GC with electron capture detection. An alternate method in which the filter and resin extracts are combined and analyzed as one may be used for some applications, including surface water trend monitoring carried out by the State of Michigan.

Section 1810: Blood Serum for PCB Congeners and Pesticides

Rev. 3.2 - August 1, 2003

1810.1 Scope and Application

This method may be used to analyze human or other blood serum for PCB congeners and chlorinated pesticides. PCB congeners included in this method are quantitated using the "Mullin 1994" mixture of Aroclors.

PCB Congeners by Capillary Column Chromatography

PCB Congener BZ # *(Ref D)	LOD (µg/L)	LOQ (µg/L)
#3	6.0	20.
#4/10	0.70	2.3
#7/9	0.15	0.50
#6	0.20	0.66
#8/5	0.40	1.3
#19	0.15	0.50
#18	0.15	0.50
#15/17	0.20	0.66
#24/27	0.15	0.50
#16/32	0.20	0.66
#26	0.15	0.50
#25	0.15	0.50
#28/31	0.30	0.99
#33	0.15	0.50
#53	0.20	0.66
#51	0.10	0.33
#22	0.20	0.66
#45	0.10	0.33
#46	0.10	0.33
#52	0.10	0.33
#49	0.10	0.33
#47/48	0.10	0.33
#44	0.10	0.33
#37/42	0.10	0.33
#41/71/64	0.15	0.50
#40	0.10	0.33
#63	0.10	0.33
#74	0.10	0.33
#70/76	0.10	0.33
#66	0.15	0.50
#95	0.10	0.33
#91	0.15	0.50
#56/60	0.10	0.33
#92/84	0.15	0.50
#89	0.10	0.33
#101	0.10	0.33
#99	0.10	0.33
#83	0.10	0.33
#97	0.10	0.33
#87	0.10	0.33
#85	0.10	0.33
#136	0.20	0.66
#77/110	0.10	0.33
#82	0.10	0.33
#151	0.10	0.33
#135/144	0.10	0.33
#123/149	0.10	0.33
#118	0.15	0.50
#146	0.10	0.33
#132/153/105	0.15	0.50
#141	0.10	0.33
#137/176	0.10	0.33
#163/138	0.15	0.50
#158	0.15	0.50
#178	0.10	0.33
#187/182	0.070	0.23
#183	0.070	0.23
#128	0.070	0.23
#167	0.10	0.33
#185	0.070	0.23
#174	0.070	0.23
#177	0.070	0.23
#202/171	0.070	0.23
#172	0.10	0.33
#180	0.10	0.33
#193	0.10	0.33
#199	0.070	0.23
#170/190	0.10	0.33
#198	0.10	0.33
#201	0.10	0.33
#203/196	0.15	0.50
#208/195	0.10	0.33
#207	0.070	0.23
#194	0.070	0.23
#206	0.070	0.23

Chlorinated Pesticides by Gas Chromatography

**Pesticides	LOD (µg/L)	LOQ (µg/L)	Report Limit (µg/L)
p,p'-DDD			5.0
p,p'-DDE	0.15	0.50
p,p'-DDT			5.0
trans nonachlor			5.0
cis nonachlor			5.0
cis chlordane			5.0

**Currently only p,p'-DDE is done on a regular basis.

Poly-Brominated Diphenyl Ethers by Capillary Column GC

BZ # (e)	Report Limit (ug/L)
#28	0.20
#47	0.25
#66	0.30
#85	0.20
#99	0.35
#100	0.20
#138	0.20
#153	0.20
#154	0.20

1810.2 Summary of Method

A portion of sample (5 mL) is extracted three times with a hexane\ethyl ether mix. The extract is then concentrated to approximately 2 mL for clean-up. Clean-up and fractionation is attained using Florisil and silica-gel. The final extract or extracts are concentrated and injected onto a gas chromatograph equipped with an electron-capture detector. The type of column and GC used varies depending on particular analytes. PCB congeners are analyzed on a 60 meter DB-5 capillary column, with confirmation on a DB-1 column.

Section 1510: Sediment and Soil for Pesticide and PCB Residues

Rev. 3.2 - August 1, 2003

1510.1 Scope and Application

This method may be used to analyze soil and sediment for various chlorinated pesticides and PCBs. Analysis for PCBs includes: Aroclor mixtures by packed column (section B, below), individual congeners contained in the "Mullin" mix by capillary/ECD (section C), and selected co-planar (or toxic) congeners by multi-dimensional GC/ECD (section D).

Pesticides by Capillary Column Chromatography

Compound	LOD(µg/g)	LOQ(µg/g)	Report Limit(µg/g)
dieldrin*	0.012	0.041
o,p-DDE			0.01
p,p-DDE	0.0050	0.016
o,p-DDD			0.01
p,p-DDD	0.010	0.033
o,p-DDT			0.01
p,p-DDT	0.014	0.045
cis-chlordane	0.0085	0.028
trans-chlordane	0.0085	0.028
cis-nonachlor	0.0085	0.028
trans-nonachlor	0.0085	0.028
aldrin			0.01
endrin	0.014	0.047
heptachlor			0.01
heptachlor epoxide			0.01
hexachlorobenzene	0.0085	0.028
alpha-BHC	0.0085	0.028
gamma-BHC	0.011	0.037
methoxychlor	0.050	0.16
toxaphene			1.0
endosulfan I			0.01
endosulfan II			0.01
endosulfan sulfate			0.01

*dieldrin is analyzed on a packed column

PCBs by Packed Column Chromatography

Aroclor	LOD (µg/g)	LOQ (µg/g)
1016	0.024	0.08
1232	0.024	0.08
1242	0.024	0.08
1248	0.024	0.08
1254	0.024	0.08
1260	0.024	0.08
1268	0.024	0.08

PCB Congeners by Capillary Column Chromatography

Sediment

BZ # (e)	Sediment LOD(ng/g)	LOQ (ng/g)
#3	6.0	19.0
#4/10	0.90	2.9
#7/9	0.20	0.64
#6	0.30	0.96
#8/5	0.60	1.9
#19	0.20	0.64
#18	0.20	0.64
#15/17	0.35	1.1
#24/27	0.30	0.96
#16/32	0.70	2.2
#26	0.30	0.96
#25	0.40	1.3
#28/31	0.40	1.3
#33	0.40	1.3
#53	0.30	0.96
#51	0.20	0.64
#22	0.30	0.96
#45	0.20	0.64
#46	0.20	0.64
#52	0.20	0.64
#49	0.15	0.48
#47/48	0.30	0.96
#44	0.20	0.64
#37/42	0.30	0.96
#41/71/64	0.30	0.96
#40	0.20	0.64
#63	0.20	0.64
#74	0.20	0.64
#70/76	0.20	0.64
#66	0.30	0.96
#95	0.20	0.64
#91	0.20	0.64
#56/60	0.30	0.96
#92/84	0.40	1.3
#89	0.30	0.96
#101	0.25	0.80
#99	0.20	0.64
#83	0.20	0.64
#97	0.20	0.64
#87	0.20	0.64
#85	0.20	0.64
#136	0.45	1.4
#77/110	0.30	0.96
#82	0.20	0.64
#151	0.20	0.64
#135/144	0.20	0.64
#123/149	0.20	0.64
#118	0.30	0.96
#146	0.30	0.96
#132/153/105	0.20	0.64
#141	0.15	0.48
#137/176	0.20	0.64
#163/138	0.30	0.96
#158	0.30	0.96
#178	0.20	0.64
#187/182	0.20	0.64
#183	0.20	0.64
#128	0.20	0.64
#167	0.30	0.96
#185	0.20	0.64
#174	0.20	0.64
#177	0.20	0.64
#202/171	0.20	0.64
#172	0.20	0.64
#180	0.20	0.64
#193	0.20	0.64
#199	0.20	0.64
#170/190	0.20	0.64
#198	0.15	0.48
#201	0.20	0.64
#203/196	0.25	0.8
#208/195	0.15	0.48
#207	0.20	0.64
#194	0.15	0.48
#206	0.15	0.48

Soil

BZ # (e)	Soil LOD (ng/g)	LOQ (ng/g)
#3	3.0	9.6
#4/10	0.50	1.6
#7/9	0.15	0.48
#6	0.20	0.64
#8/5	0.40	1.3
#19	0.15	0.48
#18	0.15	0.48
#15/17	0.20	0.64
#24/27	0.10	0.32
#16/32	0.70	2.2
#26	0.15	0.48
#25	0.15	0.48
#28/31	0.25	0.80
#33	0.15	0.48
#53	0.15	0.48
#51	0.10	0.32
#22	0.25	0.80
#45	0.10	0.32
#46	0.10	0.32
#52	0.15	0.48
#49	0.10	0.32
#47/48	0.10	0.32
#44	0.10	0.32
#37/42	0.10	0.32
#41/71/64	0.15	0.48
#40	0.10	0.32
#63	0.10	0.32
#74	0.10	0.32
#70/76	0.10	0.32
#66	0.20	0.64
#95	0.10	0.32
#91	0.15	0.48
#56/60	0.10	0.32
#92/84	0.15	0.48
#89	0.10	0.32
#101	0.20	0.64
#99	0.10	0.32
#83	0.10	0.32
#97	0.10	0.32
#87	0.10	0.32
#85	0.10	0.32
#136	0.45	1.4
#77/110	0.20	0.64
#82	0.10	0.32
#151	0.10	0.32
#135/144	0.10	0.32
#123/149	0.10	0.32
#118	0.20	0.64
#146	0.10	0.32
#132/153/105	0.20	0.64
#141	0.060	0.19
#137/176	0.10	0.32
#163/138	0.25	0.80
#158	0.15	0.48
#178	0.10	0.32
#187/182	0.080	0.26
#183	0.080	0.26
#128	0.080	0.26
#167	0.10	0.32
#185	0.080	0.26
#174	0.070	0.22
#177	0.080	0.26
#202/171	0.070	0.22
#172	0.10	0.32
#180	0.15	0.48
#193	0.10	0.32
#199	0.080	0.26
#170/190	0.080	0.26
#198	0.15	0.48
#201	0.10	0.32
#203/196	0.15	0.48
#208/195	0.070	0.22
#207	0.060	0.19
#194	0.060	0.19
#206	0.060	0.19

"Toxic" PCB Congeners by Multidimensional Gas Chromatography

NOTE: The toxic congener list includes the twelve congeners in the World Health Organization (WHO) 1998 list, plus congener #180. There is overlap with the list in Section C, which also includes congener #118, #167, and #180.

BZ # (e)	LOD (ng/g)	LOQ (ng/g)
#77	0.20	0.67
#81	0.20	0.67
#105	0.25	0.83
#114	0.20	0.67
#118	0.35	1.2
#123	0.35	1.2
#126	0.15	0.50
#156	0.25	0.83
#157	0.15	0.50
#167	0.20	0.67
#169	0.15	0.50
#180	0.30	1.0
#189	0.20	0.67

1510.2 Summary of Method

Soil or sediment samples are air dried and homogenized by sieving. The sample is then soxhlet extracted with hexane/acetone for sixteen hours. After concentrating with a roto-evaporator the extract is run through a column containing Florisil. If pesticides are of interest, a second Florisil fraction will be collected. The first fraction is concentrated and run through a column containing silica-gel. The final extract or extracts are concentrated and injected onto a gas chromatograph equipped with an electron-capture detector. The type of column and GC used varies depending on particular analytes.

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Last updated 11/13/03

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